Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805019574/rz6093sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805019574/rz6093Isup2.hkl |
CCDC reference: 277770
Data collection: COLLECT (Nonius, 2002); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1990); software used to prepare material for publication: SHELXTL.
[Fe(C12H12N2)3](ClO4)2·C12H12N2 | Z = 2 |
Mr = 991.69 | F(000) = 1032 |
Triclinic, P1 | Dx = 1.431 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.670 (2) Å | Cell parameters from 32869 reflections |
b = 13.466 (3) Å | θ = 2.7–27.5° |
c = 14.792 (3) Å | µ = 0.51 mm−1 |
α = 94.77 (3)° | T = 173 K |
β = 90.82 (3)° | Plate, red |
γ = 96.26 (3)° | 0.35 × 0.10 × 0.02 mm |
V = 2302.0 (8) Å3 |
Nonius KappaCCD diffractometer | 10528 independent reflections |
Radiation source: fine-focus sealed tube | 6461 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.108 |
ω scans | θmax = 27.5°, θmin = 2.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→15 |
Tmin = 0.842, Tmax = 0.990 | k = −17→17 |
32869 measured reflections | l = −19→19 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.078 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.238 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.130P)2 + 0.9561P] where P = (Fo2 + 2Fc2)/3 |
10528 reflections | (Δ/σ)max = 0.001 |
622 parameters | Δρmax = 0.98 e Å−3 |
18 restraints | Δρmin = −0.94 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Fe1 | 0.72986 (4) | 0.14446 (4) | 0.25751 (4) | 0.02072 (18) | |
N11 | 0.8357 (3) | 0.2596 (2) | 0.3139 (2) | 0.0217 (7) | |
C12 | 0.8028 (3) | 0.3512 (3) | 0.3022 (3) | 0.0232 (9) | |
C13 | 0.8652 (3) | 0.4398 (3) | 0.3397 (3) | 0.0276 (9) | |
H13A | 0.8402 | 0.5031 | 0.3305 | 0.033* | |
C14 | 0.9643 (4) | 0.4335 (3) | 0.3909 (3) | 0.0299 (10) | |
H14A | 1.0080 | 0.4931 | 0.4165 | 0.036* | |
C15 | 1.0001 (3) | 0.3418 (3) | 0.4049 (3) | 0.0298 (10) | |
C16 | 0.9331 (3) | 0.2566 (3) | 0.3644 (3) | 0.0276 (9) | |
H16A | 0.9573 | 0.1928 | 0.3729 | 0.033* | |
C17 | 1.1072 (4) | 0.3324 (4) | 0.4609 (4) | 0.0435 (13) | |
H17A | 1.1425 | 0.3993 | 0.4836 | 0.065* | |
H17B | 1.1621 | 0.2987 | 0.4231 | 0.065* | |
H17C | 1.0864 | 0.2930 | 0.5122 | 0.065* | |
N21 | 0.6542 (3) | 0.2550 (2) | 0.2098 (2) | 0.0203 (7) | |
C22 | 0.6979 (3) | 0.3483 (3) | 0.2449 (3) | 0.0228 (9) | |
C23 | 0.6447 (3) | 0.4326 (3) | 0.2285 (3) | 0.0285 (10) | |
H23A | 0.6758 | 0.4969 | 0.2545 | 0.034* | |
C24 | 0.5455 (4) | 0.4220 (3) | 0.1738 (3) | 0.0296 (10) | |
H24A | 0.5076 | 0.4790 | 0.1628 | 0.035* | |
C25 | 0.5020 (3) | 0.3268 (3) | 0.1350 (3) | 0.0274 (9) | |
C26 | 0.5584 (3) | 0.2462 (3) | 0.1561 (3) | 0.0251 (9) | |
H26A | 0.5281 | 0.1811 | 0.1314 | 0.030* | |
C27 | 0.3958 (4) | 0.3109 (4) | 0.0727 (3) | 0.0340 (11) | |
H27A | 0.3790 | 0.2394 | 0.0531 | 0.051* | |
H27B | 0.4100 | 0.3488 | 0.0195 | 0.051* | |
H27C | 0.3299 | 0.3342 | 0.1053 | 0.051* | |
N31 | 0.6223 (3) | 0.0359 (2) | 0.1921 (2) | 0.0220 (7) | |
C32 | 0.6533 (3) | 0.0091 (3) | 0.1066 (3) | 0.0235 (9) | |
C33 | 0.5886 (4) | −0.0673 (3) | 0.0517 (3) | 0.0309 (10) | |
H33A | 0.6114 | −0.0852 | −0.0083 | 0.037* | |
C34 | 0.4905 (4) | −0.1162 (3) | 0.0867 (3) | 0.0324 (10) | |
H34A | 0.4452 | −0.1676 | 0.0501 | 0.039* | |
C35 | 0.4581 (3) | −0.0911 (3) | 0.1743 (3) | 0.0292 (10) | |
C36 | 0.5264 (3) | −0.0125 (3) | 0.2239 (3) | 0.0271 (9) | |
H36A | 0.5035 | 0.0077 | 0.2835 | 0.033* | |
C37 | 0.3556 (4) | −0.1474 (4) | 0.2158 (4) | 0.0396 (12) | |
H37A | 0.3186 | −0.1990 | 0.1708 | 0.059* | |
H37B | 0.3002 | −0.1006 | 0.2349 | 0.059* | |
H37C | 0.3815 | −0.1792 | 0.2686 | 0.059* | |
N41 | 0.8186 (3) | 0.1266 (2) | 0.1448 (2) | 0.0224 (7) | |
C42 | 0.7622 (3) | 0.0618 (3) | 0.0783 (3) | 0.0231 (9) | |
C43 | 0.8088 (4) | 0.0459 (3) | −0.0066 (3) | 0.0297 (10) | |
H43A | 0.7667 | 0.0034 | −0.0529 | 0.036* | |
C44 | 0.9175 (4) | 0.0925 (3) | −0.0234 (3) | 0.0323 (10) | |
H44A | 0.9506 | 0.0815 | −0.0812 | 0.039* | |
C45 | 0.9777 (3) | 0.1556 (3) | 0.0449 (3) | 0.0271 (9) | |
C46 | 0.9247 (3) | 0.1711 (3) | 0.1274 (3) | 0.0230 (9) | |
H46A | 0.9647 | 0.2150 | 0.1739 | 0.028* | |
C47 | 1.0981 (4) | 0.2070 (4) | 0.0303 (3) | 0.0340 (11) | |
H47A | 1.1264 | 0.2469 | 0.0862 | 0.051* | |
H47B | 1.0951 | 0.2510 | −0.0190 | 0.051* | |
H47C | 1.1502 | 0.1563 | 0.0144 | 0.051* | |
N51 | 0.6401 (3) | 0.1492 (2) | 0.3694 (2) | 0.0223 (7) | |
C52 | 0.6762 (3) | 0.0941 (3) | 0.4354 (3) | 0.0247 (9) | |
C53 | 0.6256 (4) | 0.0938 (3) | 0.5196 (3) | 0.0306 (10) | |
H53A | 0.6533 | 0.0555 | 0.5647 | 0.037* | |
C54 | 0.5345 (4) | 0.1497 (4) | 0.5377 (3) | 0.0352 (11) | |
H54A | 0.4989 | 0.1490 | 0.5951 | 0.042* | |
C55 | 0.4946 (3) | 0.2070 (3) | 0.4720 (3) | 0.0271 (9) | |
C56 | 0.5510 (3) | 0.2039 (3) | 0.3887 (3) | 0.0243 (9) | |
H56A | 0.5252 | 0.2425 | 0.3430 | 0.029* | |
C57 | 0.3981 (4) | 0.2699 (4) | 0.4867 (3) | 0.0391 (12) | |
H57A | 0.3690 | 0.2639 | 0.5480 | 0.059* | |
H57B | 0.3359 | 0.2470 | 0.4421 | 0.059* | |
H57C | 0.4259 | 0.3401 | 0.4796 | 0.059* | |
N61 | 0.8039 (3) | 0.0436 (2) | 0.3202 (2) | 0.0219 (7) | |
C62 | 0.7698 (3) | 0.0341 (3) | 0.4067 (3) | 0.0229 (9) | |
C63 | 0.8187 (4) | −0.0284 (3) | 0.4623 (3) | 0.0328 (10) | |
H63A | 0.7947 | −0.0327 | 0.5230 | 0.039* | |
C64 | 0.9035 (4) | −0.0850 (4) | 0.4278 (4) | 0.0377 (11) | |
H64A | 0.9393 | −0.1270 | 0.4655 | 0.045* | |
C65 | 0.9357 (4) | −0.0800 (3) | 0.3381 (3) | 0.0311 (10) | |
C66 | 0.8842 (3) | −0.0134 (3) | 0.2873 (3) | 0.0267 (9) | |
H66A | 0.9070 | −0.0081 | 0.2264 | 0.032* | |
C67 | 1.02254 (19) | −0.14333 (17) | 0.29802 (17) | 0.0500 (14) | |
H67A | 1.0485 | −0.1850 | 0.3438 | 0.075* | |
H67B | 1.0886 | −0.1001 | 0.2778 | 0.075* | |
H67C | 0.9875 | −0.1865 | 0.2461 | 0.075* | |
N71 | 1.09456 (19) | −0.39381 (17) | 0.23883 (17) | 0.0402 (10) | |
C72 | 1.07515 (19) | −0.48679 (17) | 0.19626 (17) | 0.0308 (10) | |
C73 | 1.14403 (19) | −0.56191 (17) | 0.20998 (17) | 0.0360 (11) | |
H73A | 1.1265 | −0.6269 | 0.1796 | 0.043* | |
C74 | 1.2390 (4) | −0.5410 (4) | 0.2687 (4) | 0.0407 (12) | |
H74A | 1.2876 | −0.5915 | 0.2783 | 0.049* | |
C75 | 1.2625 (4) | −0.4463 (4) | 0.3130 (4) | 0.0405 (12) | |
C76 | 1.1873 (5) | −0.3770 (4) | 0.2967 (4) | 0.0498 (14) | |
H76A | 1.2017 | −0.3125 | 0.3285 | 0.060* | |
C77 | 1.3644 (5) | −0.4196 (5) | 0.3798 (5) | 0.0677 (19) | |
H77A | 1.3662 | −0.3495 | 0.4039 | 0.102* | |
H77B | 1.4363 | −0.4292 | 0.3485 | 0.102* | |
H77C | 1.3561 | −0.4631 | 0.4298 | 0.102* | |
N81 | 0.9518 (3) | −0.5978 (3) | 0.0893 (3) | 0.0365 (9) | |
C82 | 0.9701 (4) | −0.5062 (3) | 0.1337 (3) | 0.0312 (10) | |
C83 | 0.8965 (4) | −0.4336 (4) | 0.1231 (3) | 0.0375 (11) | |
H83A | 0.9118 | −0.3689 | 0.1545 | 0.045* | |
C84 | 0.8010 (4) | −0.4566 (4) | 0.0665 (3) | 0.0360 (11) | |
H84A | 0.7488 | −0.4081 | 0.0601 | 0.043* | |
C85 | 0.7802 (4) | −0.5505 (4) | 0.0184 (3) | 0.0327 (10) | |
C86 | 0.8593 (4) | −0.6179 (4) | 0.0339 (3) | 0.0399 (12) | |
H86A | 0.8465 | −0.6828 | 0.0028 | 0.048* | |
C87 | 0.6780 (4) | −0.5809 (4) | −0.0460 (4) | 0.0416 (12) | |
H87A | 0.6808 | −0.6499 | −0.0720 | 0.062* | |
H87B | 0.6806 | −0.5358 | −0.0948 | 0.062* | |
H87C | 0.6063 | −0.5766 | −0.0129 | 0.062* | |
Cl1 | 0.68163 (10) | −0.26625 (8) | 0.24199 (9) | 0.0368 (3) | |
O11 | 0.5830 (4) | −0.3282 (3) | 0.2013 (4) | 0.0729 (14) | |
O12 | 0.7531 (3) | −0.2278 (3) | 0.1723 (3) | 0.0574 (10) | |
O13 | 0.6447 (3) | −0.1838 (3) | 0.2977 (3) | 0.0472 (9) | |
O14 | 0.7471 (3) | −0.3244 (3) | 0.2961 (3) | 0.0503 (10) | |
Cl2 | 0.2480 (5) | 0.1252 (4) | 0.2634 (4) | 0.0473 (18) | 0.50 |
O21 | 0.2833 (8) | 0.2308 (4) | 0.2782 (6) | 0.076 (3) | 0.50 |
O22 | 0.2914 (9) | 0.0874 (8) | 0.1786 (6) | 0.084 (4) | 0.50 |
O23 | 0.1245 (5) | 0.1080 (8) | 0.2611 (8) | 0.137 (5) | 0.50 |
O24 | 0.2930 (10) | 0.0749 (7) | 0.3356 (6) | 0.043 (3) | 0.50 |
Cl3 | 0.2337 (4) | 0.1160 (3) | 0.2539 (3) | 0.0280 (12) | 0.50 |
O31 | 0.2066 (7) | 0.2161 (4) | 0.2772 (6) | 0.079 (4) | 0.50 |
O32 | 0.3256 (5) | 0.1182 (7) | 0.1906 (6) | 0.059 (3) | 0.50 |
O33 | 0.1338 (5) | 0.0562 (4) | 0.2137 (4) | 0.0450 (19) | 0.50 |
O34 | 0.2688 (8) | 0.0736 (7) | 0.3343 (5) | 0.072 (6) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0169 (3) | 0.0200 (3) | 0.0260 (3) | 0.0083 (2) | 0.0033 (2) | −0.0021 (2) |
N11 | 0.0154 (15) | 0.0229 (18) | 0.0275 (19) | 0.0069 (13) | 0.0048 (13) | −0.0006 (14) |
C12 | 0.0189 (18) | 0.023 (2) | 0.028 (2) | 0.0068 (16) | 0.0067 (16) | −0.0029 (17) |
C13 | 0.027 (2) | 0.026 (2) | 0.031 (2) | 0.0083 (18) | 0.0035 (17) | −0.0002 (19) |
C14 | 0.025 (2) | 0.031 (2) | 0.033 (2) | 0.0039 (18) | 0.0032 (18) | −0.0022 (19) |
C15 | 0.020 (2) | 0.036 (3) | 0.034 (3) | 0.0063 (18) | −0.0020 (17) | 0.001 (2) |
C16 | 0.024 (2) | 0.029 (2) | 0.031 (2) | 0.0101 (18) | 0.0009 (17) | 0.0032 (19) |
C17 | 0.026 (2) | 0.047 (3) | 0.057 (3) | 0.003 (2) | −0.012 (2) | 0.004 (3) |
N21 | 0.0167 (15) | 0.0228 (18) | 0.0223 (18) | 0.0083 (13) | 0.0047 (13) | −0.0016 (14) |
C22 | 0.0210 (19) | 0.023 (2) | 0.025 (2) | 0.0078 (16) | 0.0044 (16) | −0.0024 (17) |
C23 | 0.023 (2) | 0.020 (2) | 0.042 (3) | 0.0068 (17) | 0.0005 (18) | −0.0029 (19) |
C24 | 0.027 (2) | 0.021 (2) | 0.042 (3) | 0.0114 (17) | 0.0010 (19) | 0.0025 (19) |
C25 | 0.0194 (19) | 0.024 (2) | 0.040 (3) | 0.0064 (17) | 0.0030 (17) | 0.0028 (19) |
C26 | 0.0203 (19) | 0.024 (2) | 0.031 (2) | 0.0078 (17) | 0.0027 (17) | 0.0001 (18) |
C27 | 0.024 (2) | 0.033 (3) | 0.047 (3) | 0.0124 (19) | −0.0065 (19) | 0.002 (2) |
N31 | 0.0221 (16) | 0.0174 (17) | 0.0274 (19) | 0.0077 (14) | 0.0036 (14) | −0.0021 (14) |
C32 | 0.0190 (18) | 0.021 (2) | 0.031 (2) | 0.0067 (16) | 0.0021 (16) | −0.0021 (17) |
C33 | 0.031 (2) | 0.029 (2) | 0.031 (2) | 0.0072 (19) | 0.0013 (18) | −0.0083 (19) |
C34 | 0.030 (2) | 0.027 (2) | 0.037 (3) | −0.0020 (19) | −0.0026 (19) | −0.009 (2) |
C35 | 0.024 (2) | 0.024 (2) | 0.039 (3) | 0.0060 (17) | 0.0016 (18) | −0.0023 (19) |
C36 | 0.025 (2) | 0.027 (2) | 0.030 (2) | 0.0068 (18) | 0.0032 (17) | −0.0009 (19) |
C37 | 0.029 (2) | 0.038 (3) | 0.049 (3) | −0.006 (2) | 0.006 (2) | −0.004 (2) |
N41 | 0.0213 (16) | 0.0166 (17) | 0.0298 (19) | 0.0063 (13) | 0.0022 (14) | −0.0005 (14) |
C42 | 0.0239 (19) | 0.019 (2) | 0.028 (2) | 0.0074 (16) | 0.0048 (16) | −0.0012 (17) |
C43 | 0.028 (2) | 0.032 (2) | 0.029 (2) | 0.0075 (19) | 0.0030 (18) | −0.0039 (19) |
C44 | 0.035 (2) | 0.034 (3) | 0.029 (2) | 0.012 (2) | 0.0115 (19) | −0.002 (2) |
C45 | 0.023 (2) | 0.027 (2) | 0.032 (2) | 0.0075 (17) | 0.0062 (17) | 0.0009 (19) |
C46 | 0.0181 (18) | 0.025 (2) | 0.027 (2) | 0.0076 (16) | 0.0045 (16) | −0.0005 (17) |
C47 | 0.024 (2) | 0.040 (3) | 0.039 (3) | 0.0082 (19) | 0.0118 (19) | 0.003 (2) |
N51 | 0.0186 (16) | 0.0197 (17) | 0.0286 (19) | 0.0073 (13) | 0.0038 (13) | −0.0045 (14) |
C52 | 0.025 (2) | 0.020 (2) | 0.029 (2) | 0.0053 (17) | 0.0031 (17) | −0.0013 (17) |
C53 | 0.034 (2) | 0.032 (2) | 0.028 (2) | 0.013 (2) | 0.0054 (18) | 0.0027 (19) |
C54 | 0.033 (2) | 0.041 (3) | 0.033 (3) | 0.014 (2) | 0.0136 (19) | −0.002 (2) |
C55 | 0.022 (2) | 0.027 (2) | 0.032 (2) | 0.0058 (17) | 0.0045 (17) | −0.0040 (19) |
C56 | 0.0211 (19) | 0.024 (2) | 0.028 (2) | 0.0103 (17) | 0.0039 (16) | −0.0023 (18) |
C57 | 0.031 (2) | 0.049 (3) | 0.040 (3) | 0.022 (2) | 0.009 (2) | −0.002 (2) |
N61 | 0.0191 (16) | 0.0189 (17) | 0.0275 (19) | 0.0053 (13) | 0.0021 (13) | −0.0044 (14) |
C62 | 0.025 (2) | 0.019 (2) | 0.025 (2) | 0.0064 (16) | 0.0037 (16) | −0.0023 (17) |
C63 | 0.035 (2) | 0.033 (3) | 0.033 (3) | 0.013 (2) | 0.0042 (19) | 0.004 (2) |
C64 | 0.034 (2) | 0.034 (3) | 0.049 (3) | 0.016 (2) | 0.002 (2) | 0.008 (2) |
C65 | 0.031 (2) | 0.025 (2) | 0.041 (3) | 0.0150 (19) | 0.0054 (19) | 0.002 (2) |
C66 | 0.025 (2) | 0.019 (2) | 0.037 (3) | 0.0091 (17) | 0.0070 (18) | −0.0012 (18) |
C67 | 0.048 (3) | 0.047 (3) | 0.062 (4) | 0.033 (3) | 0.012 (3) | 0.007 (3) |
N71 | 0.038 (2) | 0.028 (2) | 0.055 (3) | 0.0060 (18) | −0.0007 (19) | −0.0028 (19) |
C72 | 0.028 (2) | 0.028 (2) | 0.038 (3) | 0.0061 (18) | 0.0113 (19) | 0.004 (2) |
C73 | 0.033 (2) | 0.032 (3) | 0.044 (3) | 0.010 (2) | 0.002 (2) | −0.003 (2) |
C74 | 0.031 (2) | 0.043 (3) | 0.050 (3) | 0.011 (2) | 0.005 (2) | 0.003 (2) |
C75 | 0.034 (2) | 0.032 (3) | 0.055 (3) | 0.004 (2) | −0.005 (2) | 0.002 (2) |
C76 | 0.050 (3) | 0.028 (3) | 0.070 (4) | 0.003 (2) | −0.003 (3) | −0.002 (3) |
C77 | 0.054 (4) | 0.053 (4) | 0.093 (5) | 0.004 (3) | −0.022 (3) | −0.003 (3) |
N81 | 0.036 (2) | 0.031 (2) | 0.044 (2) | 0.0158 (17) | 0.0007 (18) | −0.0042 (18) |
C82 | 0.029 (2) | 0.030 (2) | 0.036 (3) | 0.0076 (19) | 0.0139 (19) | 0.004 (2) |
C83 | 0.035 (2) | 0.030 (3) | 0.048 (3) | 0.013 (2) | 0.009 (2) | 0.000 (2) |
C84 | 0.029 (2) | 0.032 (3) | 0.050 (3) | 0.016 (2) | 0.003 (2) | 0.007 (2) |
C85 | 0.028 (2) | 0.034 (3) | 0.037 (3) | 0.008 (2) | 0.0090 (19) | 0.006 (2) |
C86 | 0.045 (3) | 0.030 (3) | 0.045 (3) | 0.012 (2) | 0.000 (2) | −0.004 (2) |
C87 | 0.035 (2) | 0.039 (3) | 0.053 (3) | 0.009 (2) | 0.001 (2) | 0.010 (2) |
Cl1 | 0.0362 (6) | 0.0280 (6) | 0.0476 (7) | 0.0125 (5) | 0.0107 (5) | −0.0009 (5) |
O11 | 0.057 (2) | 0.045 (2) | 0.113 (4) | −0.003 (2) | −0.017 (3) | −0.001 (2) |
O12 | 0.064 (2) | 0.055 (2) | 0.057 (3) | 0.018 (2) | 0.028 (2) | 0.007 (2) |
O13 | 0.054 (2) | 0.037 (2) | 0.054 (2) | 0.0242 (17) | 0.0200 (17) | −0.0034 (17) |
O14 | 0.061 (2) | 0.043 (2) | 0.053 (2) | 0.0271 (18) | 0.0073 (18) | 0.0068 (18) |
Cl2 | 0.042 (3) | 0.047 (3) | 0.051 (3) | 0.016 (2) | −0.010 (2) | −0.013 (2) |
O21 | 0.134 (10) | 0.038 (5) | 0.060 (6) | 0.029 (6) | 0.010 (7) | 0.012 (4) |
O22 | 0.123 (8) | 0.080 (7) | 0.047 (6) | 0.040 (6) | −0.010 (6) | −0.035 (5) |
O23 | 0.073 (7) | 0.147 (9) | 0.196 (10) | 0.012 (7) | 0.000 (7) | 0.054 (8) |
O24 | 0.047 (5) | 0.045 (8) | 0.041 (8) | 0.026 (4) | 0.012 (4) | 0.010 (6) |
Cl3 | 0.0253 (17) | 0.0249 (19) | 0.036 (2) | 0.0088 (14) | 0.0041 (15) | 0.0068 (16) |
O31 | 0.105 (7) | 0.052 (5) | 0.081 (6) | 0.047 (5) | −0.029 (6) | −0.031 (4) |
O32 | 0.019 (3) | 0.109 (9) | 0.057 (6) | 0.006 (5) | 0.016 (4) | 0.044 (6) |
O33 | 0.048 (4) | 0.043 (4) | 0.039 (4) | −0.010 (4) | −0.012 (3) | −0.006 (3) |
O34 | 0.102 (11) | 0.074 (11) | 0.039 (9) | 0.001 (7) | −0.020 (7) | 0.018 (8) |
Fe1—N51 | 1.972 (4) | C52—C62 | 1.474 (6) |
Fe1—N61 | 1.973 (3) | C53—C54 | 1.385 (6) |
Fe1—N21 | 1.983 (3) | C53—H53A | 0.9500 |
Fe1—N41 | 1.987 (4) | C54—C55 | 1.395 (6) |
Fe1—N11 | 1.991 (3) | C54—H54A | 0.9500 |
Fe1—N31 | 1.995 (3) | C55—C56 | 1.404 (6) |
N11—C12 | 1.355 (5) | C55—C57 | 1.489 (6) |
N11—C16 | 1.358 (5) | C56—H56A | 0.9500 |
C12—C13 | 1.397 (6) | C57—H57A | 0.9800 |
C12—C22 | 1.474 (5) | C57—H57B | 0.9800 |
C13—C14 | 1.387 (6) | C57—H57C | 0.9800 |
C13—H13A | 0.9500 | N61—C66 | 1.347 (5) |
C14—C15 | 1.377 (6) | N61—C62 | 1.358 (5) |
C14—H14A | 0.9500 | C62—C63 | 1.385 (6) |
C15—C16 | 1.401 (6) | C63—C64 | 1.390 (6) |
C15—C17 | 1.512 (6) | C63—H63A | 0.9500 |
C16—H16A | 0.9500 | C64—C65 | 1.389 (7) |
C17—H17A | 0.9800 | C64—H64A | 0.9500 |
C17—H17B | 0.9800 | C65—C66 | 1.394 (6) |
C17—H17C | 0.9800 | C65—C67 | 1.493 (5) |
N21—C26 | 1.351 (5) | C66—H66A | 0.9500 |
N21—C22 | 1.361 (5) | C67—H67A | 0.9800 |
C22—C23 | 1.388 (6) | C67—H67B | 0.9800 |
C23—C24 | 1.391 (6) | C67—H67C | 0.9800 |
C23—H23A | 0.9500 | N71—C72 | 1.349 (3) |
C24—C25 | 1.399 (6) | N71—C76 | 1.358 (6) |
C24—H24A | 0.9500 | C72—C73 | 1.384 (3) |
C25—C26 | 1.384 (6) | C72—C82 | 1.512 (5) |
C25—C27 | 1.519 (6) | C73—C74 | 1.387 (5) |
C26—H26A | 0.9500 | C73—H73A | 0.9500 |
C27—H27A | 0.9800 | C74—C75 | 1.383 (7) |
C27—H27B | 0.9800 | C74—H74A | 0.9500 |
C27—H27C | 0.9800 | C75—C76 | 1.382 (7) |
N31—C36 | 1.344 (5) | C75—C77 | 1.527 (7) |
N31—C32 | 1.352 (5) | C76—H76A | 0.9500 |
C32—C33 | 1.401 (6) | C77—H77A | 0.9800 |
C32—C42 | 1.470 (6) | C77—H77B | 0.9800 |
C33—C34 | 1.386 (6) | C77—H77C | 0.9800 |
C33—H33A | 0.9500 | N81—C86 | 1.335 (6) |
C34—C35 | 1.380 (6) | N81—C82 | 1.343 (6) |
C34—H34A | 0.9500 | C82—C83 | 1.387 (6) |
C35—C36 | 1.402 (6) | C83—C84 | 1.377 (7) |
C35—C37 | 1.511 (6) | C83—H83A | 0.9500 |
C36—H36A | 0.9500 | C84—C85 | 1.393 (7) |
C37—H37A | 0.9800 | C84—H84A | 0.9500 |
C37—H37B | 0.9800 | C85—C86 | 1.392 (6) |
C37—H37C | 0.9800 | C85—C87 | 1.515 (6) |
N41—C46 | 1.353 (5) | C86—H86A | 0.9500 |
N41—C42 | 1.369 (5) | C87—H87A | 0.9800 |
C42—C43 | 1.385 (6) | C87—H87B | 0.9800 |
C43—C44 | 1.388 (6) | C87—H87C | 0.9800 |
C43—H43A | 0.9500 | Cl1—O12 | 1.431 (4) |
C44—C45 | 1.393 (6) | Cl1—O14 | 1.433 (4) |
C44—H44A | 0.9500 | Cl1—O13 | 1.435 (3) |
C45—C46 | 1.387 (6) | Cl1—O11 | 1.439 (4) |
C45—C47 | 1.523 (6) | Cl2—O22 | 1.4339 |
C46—H46A | 0.9500 | Cl2—O23 | 1.4340 |
C47—H47A | 0.9800 | Cl2—O21 | 1.4340 |
C47—H47B | 0.9800 | Cl2—O24 | 1.4340 |
C47—H47C | 0.9800 | Cl3—O32 | 1.4339 |
N51—C56 | 1.360 (5) | Cl3—O31 | 1.4340 |
N51—C52 | 1.363 (5) | Cl3—O33 | 1.4340 |
C52—C53 | 1.385 (6) | Cl3—O34 | 1.4340 |
N51—Fe1—N61 | 81.75 (14) | C56—N51—C52 | 117.5 (4) |
N51—Fe1—N21 | 92.40 (14) | C56—N51—Fe1 | 127.3 (3) |
N61—Fe1—N21 | 172.76 (14) | C52—N51—Fe1 | 115.1 (3) |
N51—Fe1—N41 | 174.93 (13) | N51—C52—C53 | 122.0 (4) |
N61—Fe1—N41 | 94.54 (14) | N51—C52—C62 | 113.3 (4) |
N21—Fe1—N41 | 91.55 (14) | C53—C52—C62 | 124.7 (4) |
N51—Fe1—N11 | 88.26 (14) | C52—C53—C54 | 119.7 (4) |
N61—Fe1—N11 | 94.09 (13) | C52—C53—H53A | 120.2 |
N21—Fe1—N11 | 81.42 (13) | C54—C53—H53A | 120.2 |
N41—Fe1—N11 | 95.48 (14) | C53—C54—C55 | 120.2 (4) |
N51—Fe1—N31 | 94.61 (14) | C53—C54—H54A | 119.9 |
N61—Fe1—N31 | 90.17 (13) | C55—C54—H54A | 119.9 |
N21—Fe1—N31 | 94.56 (13) | C54—C55—C56 | 116.7 (4) |
N41—Fe1—N31 | 81.90 (14) | C54—C55—C57 | 123.4 (4) |
N11—Fe1—N31 | 175.17 (14) | C56—C55—C57 | 119.9 (4) |
C12—N11—C16 | 117.2 (4) | N51—C56—C55 | 124.0 (4) |
C12—N11—Fe1 | 114.9 (3) | N51—C56—H56A | 118.0 |
C16—N11—Fe1 | 127.8 (3) | C55—C56—H56A | 118.0 |
N11—C12—C13 | 122.4 (4) | C55—C57—H57A | 109.5 |
N11—C12—C22 | 113.9 (3) | C55—C57—H57B | 109.5 |
C13—C12—C22 | 123.7 (4) | H57A—C57—H57B | 109.5 |
C14—C13—C12 | 118.7 (4) | C55—C57—H57C | 109.5 |
C14—C13—H13A | 120.7 | H57A—C57—H57C | 109.5 |
C12—C13—H13A | 120.7 | H57B—C57—H57C | 109.5 |
C15—C14—C13 | 120.7 (4) | C66—N61—C62 | 118.1 (4) |
C15—C14—H14A | 119.7 | C66—N61—Fe1 | 127.4 (3) |
C13—C14—H14A | 119.7 | C62—N61—Fe1 | 114.5 (3) |
C14—C15—C16 | 117.1 (4) | N61—C62—C63 | 122.0 (4) |
C14—C15—C17 | 121.9 (4) | N61—C62—C52 | 114.7 (3) |
C16—C15—C17 | 121.0 (4) | C63—C62—C52 | 123.3 (4) |
N11—C16—C15 | 124.0 (4) | C62—C63—C64 | 119.1 (4) |
N11—C16—H16A | 118.0 | C62—C63—H63A | 120.5 |
C15—C16—H16A | 118.0 | C64—C63—H63A | 120.5 |
C15—C17—H17A | 109.5 | C65—C64—C63 | 119.8 (4) |
C15—C17—H17B | 109.5 | C65—C64—H64A | 120.1 |
H17A—C17—H17B | 109.5 | C63—C64—H64A | 120.1 |
C15—C17—H17C | 109.5 | C64—C65—C66 | 117.5 (4) |
H17A—C17—H17C | 109.5 | C64—C65—C67 | 121.1 (4) |
H17B—C17—H17C | 109.5 | C66—C65—C67 | 121.4 (4) |
C26—N21—C22 | 118.1 (3) | N61—C66—C65 | 123.4 (4) |
C26—N21—Fe1 | 127.0 (3) | N61—C66—H66A | 118.3 |
C22—N21—Fe1 | 114.4 (2) | C65—C66—H66A | 118.3 |
N21—C22—C23 | 121.6 (4) | C65—C67—H67A | 109.5 |
N21—C22—C12 | 114.7 (3) | C65—C67—H67B | 109.5 |
C23—C22—C12 | 123.7 (4) | H67A—C67—H67B | 109.5 |
C22—C23—C24 | 119.5 (4) | C65—C67—H67C | 109.5 |
C22—C23—H23A | 120.3 | H67A—C67—H67C | 109.5 |
C24—C23—H23A | 120.3 | H67B—C67—H67C | 109.5 |
C23—C24—C25 | 119.4 (4) | C72—N71—C76 | 115.9 (2) |
C23—C24—H24A | 120.3 | N71—C72—C73 | 123.0 (2) |
C25—C24—H24A | 120.3 | N71—C72—C82 | 115.89 (19) |
C26—C25—C24 | 117.7 (4) | C73—C72—C82 | 121.07 (19) |
C26—C25—C27 | 120.4 (4) | C72—C73—C74 | 119.1 (2) |
C24—C25—C27 | 121.9 (4) | C72—C73—H73A | 120.4 |
N21—C26—C25 | 123.7 (4) | C74—C73—H73A | 120.4 |
N21—C26—H26A | 118.2 | C75—C74—C73 | 119.6 (4) |
C25—C26—H26A | 118.2 | C75—C74—H74A | 120.2 |
C25—C27—H27A | 109.5 | C73—C74—H74A | 120.2 |
C25—C27—H27B | 109.5 | C76—C75—C74 | 117.0 (4) |
H27A—C27—H27B | 109.5 | C76—C75—C77 | 121.0 (5) |
C25—C27—H27C | 109.5 | C74—C75—C77 | 121.9 (5) |
H27A—C27—H27C | 109.5 | N71—C76—C75 | 125.2 (5) |
H27B—C27—H27C | 109.5 | N71—C76—H76A | 117.4 |
C36—N31—C32 | 118.3 (3) | C75—C76—H76A | 117.4 |
C36—N31—Fe1 | 127.5 (3) | C75—C77—H77A | 109.5 |
C32—N31—Fe1 | 114.2 (3) | C75—C77—H77B | 109.5 |
N31—C32—C33 | 121.6 (4) | H77A—C77—H77B | 109.5 |
N31—C32—C42 | 115.1 (3) | C75—C77—H77C | 109.5 |
C33—C32—C42 | 123.2 (4) | H77A—C77—H77C | 109.5 |
C34—C33—C32 | 118.6 (4) | H77B—C77—H77C | 109.5 |
C34—C33—H33A | 120.7 | C86—N81—C82 | 117.9 (4) |
C32—C33—H33A | 120.7 | N81—C82—C83 | 121.9 (4) |
C35—C34—C33 | 120.7 (4) | N81—C82—C72 | 116.3 (4) |
C35—C34—H34A | 119.6 | C83—C82—C72 | 121.8 (4) |
C33—C34—H34A | 119.6 | C84—C83—C82 | 119.0 (5) |
C34—C35—C36 | 117.0 (4) | C84—C83—H83A | 120.5 |
C34—C35—C37 | 121.7 (4) | C82—C83—H83A | 120.5 |
C36—C35—C37 | 121.4 (4) | C83—C84—C85 | 120.6 (4) |
N31—C36—C35 | 123.7 (4) | C83—C84—H84A | 119.7 |
N31—C36—H36A | 118.2 | C85—C84—H84A | 119.7 |
C35—C36—H36A | 118.2 | C86—C85—C84 | 115.8 (4) |
C35—C37—H37A | 109.5 | C86—C85—C87 | 120.6 (4) |
C35—C37—H37B | 109.5 | C84—C85—C87 | 123.6 (4) |
H37A—C37—H37B | 109.5 | N81—C86—C85 | 124.8 (4) |
C35—C37—H37C | 109.5 | N81—C86—H86A | 117.6 |
H37A—C37—H37C | 109.5 | C85—C86—H86A | 117.6 |
H37B—C37—H37C | 109.5 | C85—C87—H87A | 109.5 |
C46—N41—C42 | 118.3 (4) | C85—C87—H87B | 109.5 |
C46—N41—Fe1 | 127.7 (3) | H87A—C87—H87B | 109.5 |
C42—N41—Fe1 | 114.0 (3) | C85—C87—H87C | 109.5 |
N41—C42—C43 | 121.4 (4) | H87A—C87—H87C | 109.5 |
N41—C42—C32 | 114.4 (4) | H87B—C87—H87C | 109.5 |
C43—C42—C32 | 124.2 (4) | O12—Cl1—O14 | 108.9 (2) |
C42—C43—C44 | 119.5 (4) | O12—Cl1—O13 | 109.0 (2) |
C42—C43—H43A | 120.3 | O14—Cl1—O13 | 109.7 (2) |
C44—C43—H43A | 120.3 | O12—Cl1—O11 | 109.5 (3) |
C43—C44—C45 | 119.7 (4) | O14—Cl1—O11 | 109.8 (2) |
C43—C44—H44A | 120.2 | O13—Cl1—O11 | 109.9 (2) |
C45—C44—H44A | 120.2 | O22—Cl2—O23 | 109.5 |
C46—C45—C44 | 118.0 (4) | O22—Cl2—O21 | 109.4 |
C46—C45—C47 | 120.3 (4) | O23—Cl2—O21 | 109.4 |
C44—C45—C47 | 121.7 (4) | O22—Cl2—O24 | 109.5 |
N41—C46—C45 | 123.0 (4) | O23—Cl2—O24 | 109.5 |
N41—C46—H46A | 118.5 | O21—Cl2—O24 | 109.4 |
C45—C46—H46A | 118.5 | O32—Cl3—O31 | 109.4 |
C45—C47—H47A | 109.5 | O32—Cl3—O33 | 109.5 |
C45—C47—H47B | 109.5 | O31—Cl3—O33 | 109.4 |
H47A—C47—H47B | 109.5 | O32—Cl3—O34 | 109.5 |
C45—C47—H47C | 109.5 | O31—Cl3—O34 | 109.4 |
H47A—C47—H47C | 109.5 | O33—Cl3—O34 | 109.5 |
H47B—C47—H47C | 109.5 |